A novel 2-D supramolecular network formed by the Fe3O building unit through three hydrogen bonds [Fe3O(O2CCH2OC6H5)6(3H2O)]NO3·2H2O (1) are presented. The title complex crystallizes in monoclinic, space group P21/n, with a=1.709 3(2) nm, b=3.152 9(3) nm, c=1.021 2(2) nm, V=5.503 5(14) nm3, Z=4, D(calc)=1.500 g·cm-3, F(000)=2 564. Each Fe3O unit is connected by three NO3-ions and inversely each NO3-ion is surrounded by three Fe3O moieties. It shows that the well-known Fe3O unit is a potential three H-donors and may be able to be a three-connected linker. This complex displays weak anti-ferromagnetic coupling between Fe(Ⅲ) centers. Electrochemical experiments were carried out to obtain the character of its redox reaction. CCDC: 222011.
